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Review of Green Food Processing techniques.Preservation, transformation, and extraction

Farid Chemat, Natacha Rombaut, Alice Meullemiestre, Mohammad Turk,Sandrine Périno-Issartier, Anne-Sylvie Fabiano-Tixier, Maryline Vian

To cite this version:Farid Chemat, Natacha Rombaut, Alice Meullemiestre, Mohammad Turk, Sandrine Périno-Issartier,et al.. Review of Green Food Processing techniques. Preservation, transformation, and ex-traction. Innovative Food Science and Emerging Technologies, Elsevier, 2017, 41, pp.357-377.�10.1016/j.ifset.2017.04.016�. �hal-01552142�

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Comment citer ce document :Chemat, F. (Auteur de correspondance), Rombaut, N., Meullemiestre, A., Turk, M., Périno, S.,Fabiano-Tixier, A.-S., Abert-Vian, M. (2017). Review of Green Food Processing techniques.

Preservation, transformation, and extraction. Innovative Food Science and Emerging Technologies, 41,357-377. DOI : 10.1016/j.ifset.2017.04.016

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Version définitive du manuscrit publiée dans / Final version of the manuscript published in : Innovative Food Science and Emerging Technologies (2017), Vol. 41, p. 357-377, DOI: 10.1016/j.ifset.2017.04.016, Journal homepage : http://www.elsevier.com/locate/ifset

Review of Green Food Processing techniques. Preservation, transformation,and extraction

Farid Chemat⁎, Natacha Rombaut, Alice Meullemiestre, Mohammad Turk, Sandrine Perino,Anne-Sylvie Fabiano-Tixier, Maryline Abert-VianUniversité d'Avignon et des Pays de Vaucluse, INRA, UMR408, GREEN Team Extraction, F-84000 Avignon, France

A R T I C L E I N F O

Keywords:Green Food ProcessingPreservationTransformationExtractionInnovative techniquesIntensificationBio-refinery

A B S T R A C T

This review presents innovative food processing techniques and their role in promoting sustainable foodindustry. These techniques (such as microwave, ultrasound, pulse electric field, instant controlled pressure drop,supercritical fluid processing) in the frontiers of food processing, food chemistry, and food microbiology, are notnew and were already used for> 30 years by academia and industry. We will pay special attention to thestrategies and the tools available to make preservation, transformation and extraction greener and present themas success stories for research, education and at industrial scale. The design of green and sustainable processes iscurrently a hot research topic in food industry. Herein we aimed to describe a multifaceted strategy (innovativetechnologies, process intensification, bio-refinery concept) to apply this concept at research, educational, andindustrial level.Industrial relevance: Green Food Processing could be a new concept to meet the challenges of the 21st century, toprotect both the environment and consumers, and in the meantime enhance competition of industries to be moreecologic, economic and innovative. This green approach should be the result of a whole chain of values in bothsenses of the term: economic and responsible, starting from the production and harvesting of food raw materials,processes of preservation, transformation, and extraction together with formulation and marketing.

1. Introduction

Food products, such as fruit and vegetables, fat and oils, sugar,dairy, meat, coffee and cocoa, meal and flours, are complex mixtures ofvitamins, sugars, proteins and lipids, fibres, aromas, pigments, anti-oxidants, and other organic and mineral compounds. Before suchproducts can be commercialized, they have to be processed andpreserved for food ready meals and extracted for food ingredients.Different methods can be used for this purpose, e.g. frying, drying,filtering, and cooking. Nevertheless, many food ingredients and pro-ducts are well known to be thermally sensitive and vulnerable tochemical, physical and microbiological changes. Losses of some nutri-tional compounds, low production efficiency, time- and energy-con-suming procedures (prolonged heating and stirring, use of largevolumes of water…) may be encountered using these conventionalfood-processing methods. These shortcomings have led to the use ofnew sustainable “green and innovative” techniques in processing,pasteurization and extraction, which typically involve less time, waterand energy, such as ultrasound-assisted processing, supercritical fluidextraction and processing, microwave processing, controlled pressure

drop process, and pulse electric field. The tremendous efforts made ongreening food process can be evaluated through the consideration ofbooks and journals devoted to these aspects (Chemat, Huma, & Khan,2011).

Food technology under extreme or non-classical conditions iscurrently a dynamically developing area in applied research andindustry. Alternatives to conventional processing, preservation andextraction procedures may increase production efficiency and contri-bute to environmental preservation by reducing the use of water andsolvents, elimination of wastewater, fossil energy and generation ofhazardous substances. Within those constraints, “Green FoodProcessing” has to be introduced on the basis of green chemistry andgreen engineering: “Green Food Processing is based on the discovery anddesign of technical processes which will reduce energy and water consump-tion, allows recycling of by-products through bio-refinery, and ensure a safeand high quality product” (Fig. 1).

This review presents a complete picture of current knowledge onGreen Food Processing techniques for preservation, transformation andextraction as success stories for research, education and at industrialscale. The readers like chemists, biochemists, chemical engineers,

http://dx.doi.org/10.1016/j.ifset.2017.04.016Received 16 November 2016; Received in revised form 23 February 2017; Accepted 30 April 2017

⁎ Corresponding author.E-mail address: [email protected] (F. Chemat).

Available online 03 May 20171466-8564/ © 2017 Elsevier Ltd. All rights reserved.

http://www.sciencedirect.com/science/journal/14668564

http://www.elsevier.com/locate/ifset

http://dx.doi.org/10.1016/j.ifset.2017.04.016


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physicians, and food technologists even from academia or industry willfind the major solutions identified to design and demonstrate GreenFood Processing on laboratory, classroom and industrial scale toapproach an optimal consumption of raw food materials, water andenergy: (1) improving and optimization of existing processes; (2) usingnon-dedicated equipment; and (3) innovation in processes and proce-dures.

2. Instant controlled pressure drop technology

2.1. Process and procedure

DIC ‘Détente Instantanée Contrôlée’, French for Instant ControlledPressure-Drop is based on the main principle of the thermodynamics ofinstantaneity and auto-vaporization processing combining with hydro-

intensification

ClassicalToday’s

US

MW

DIC

PEF

CO2

Processing yield

Processing time

Product price

Reduction of Energy

Recycling of by products

Product quality HACCP

Reduction of Water use

Process safety HAZOP

Carbon and water footprint

Fig. 1. Green Food Processing: evolution or revolution.

Fig. 2. Schematic representation (a) and photography (b) of DIC process, from experimental conditions (c) to an example of a major macroscopic (d) and microscopic (e) phenomenagenerated by DIC treatment.

F. Chemat et al. Innovative Food Science and Emerging Technologies 41 (2017) 357–377

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Version définitive du manuscrit publiée dans / Final version of the manuscript published in : Innovative Food Science and Emerging Technologies (2017), Vol. 41, p. 357-377, DOI: 10.1016/j.ifset.2017.04.016, Journal homepage : http://www.elsevier.com/locate/ifsetthermo-mechanical evolution of many biopolymers for food, cosmetic,and pharmaceutical purposes. Developed by Allaf and Vidal (1989),DIC's research began by fundamental studies regarding expansionthrough alveolation and has targeted several applications in responseto issues of control and quality improvement. DIC is considered as ahigh temperature/high pressure - short time (HTST) treatment andconsists of thermo-mechanical processing induced by subjecting theraw material to saturated steam for a short period, and followed by anabrupt pressure drop towards vacuum (about 5 kPa with a rate > 0.5MPa.s−1). Typically, the sample was adjusted to about 30% dry basisand submitted to a first pressure drop in the treatment vessel to be pre-conditioned. Then, the sample is subjected to heating under highsaturated pressure (up to 1 MPa) at high temperature (up to 180 °C)during a short time (5 to 60 s) and followed by an abrupt pressure dropto vacuum (3–5 kPa, Δt = 20–200 ms). The abrupt pressure drop (ΔP/Δt > 25.106 Pa.s−1) induces a significant mechanical stress related toinstant auto-vaporization of water, an instantaneous cooling of thesample, and swelling phenomenon, causing the rupture of cells andsecretion of metabolites through cell walls (Allaf et al., 2011). Thepurpose of these effects leads to texture change, which results in higherporosity, as well as increased specific surface area and reduceddiffusion resistance of the sample. Experimental conditions of DICextraction allow reduced processing time and the instant reducingtemperature drops prevent further thermal deterioration and ensure ahigh quality of extract (Haddad, Louka, Gadouleau, Juhel, & Allaf,2001)

DIC equipment is composed of four major components (Fig. 2): (1)an extraction vessel, which is an autoclave with a heating jacket wherethe sample to be treated is placed; (2) a controlled pressure-drop valve,which ensures a quick and controlled liberation of steam pressurecontained in the extraction vessel to the vacuum pump; (3) a vacuumsystem composed of a vacuum pump and a tank with a volume 50-foldhigher than the volume of the treatment vessel; (4) an extract collectiontrap used to recover condensates; a water ring pump maintains the tankpressure at about 5 kPa. At the beginning, humidified product is placedin the autoclave at atmospheric pressure before vacuum setting. Initialvacuum ensures closer contact of the fluid heating with the exchangesurface, which enhances the heat transfer in raw material. After closingthe valve (between the autoclave and the vacuum tank), the autoclaveis filled with steam up to a processing pressure. After this treatmenttime, the controlled pressure-drop valve is instantaneously opened(in< 200 ms), resulting in an abrupt pressure drop inside the treat-ment vessel. After steam release, the atmospheric pressure is returnedback inside the reactor.

2.2. Applications in food processing

DIC treatment is employed in several industrial fields such as food,cosmetic, pharmaceutic in response to issues of control and qualityimprovement, coupled with reduced energy costs (Allaf & Allaf, 2014).As shown in Table 1, DIC can be used in various operations such astransformation, preservation, and extraction. For each operation theapproach has always induced the integration of phenomena of instan-taneity to intensify the elementary processes of transfer.

The DIC treatment combined to classical hot air drying may beconsidered as the tool of intensifying the drying when the kinetics ofdehydration is particularly low due to difficulty of water transferthrough material because of resistance of the natural structure of thematerial. Recently, Mounir and Allaf (2008) propose an innovativeprocess of 3-stage spray-drying using DIC treatment of powders (sodiumcaseinates, whey proteins), using saturated steam as a texturing fluidwhich can permit the modification of powder granule structure, andallows the formation of vacuoles and pores. DIC increases the specificsurface area of spray-dried powder and consequently overcomes theproblems related to the presence of fine powder (dustiness). DICtreatment appears to be a good alternative to expand granule powder

of heat-sensitive food such as apple and onion (Mounir, Besombes, Al-Bitar, & Allaf, 2011). After an initial partial drying step, DIC treatmentpermits the improvement of dehydration kinetic inserting a texturingprocess allowing the partially dried product to be expanded. The secondstep of drying (after DIC treatment) is greatly reduced from 6 h(untreated apple) to 1 h in the case of treated-sample. In the case ofonion, the effective diffusivity is accelerated after DIC treatment(7.56·10−10 as against 0.46·10−10 m2·s−1 for untreated sample. Atequal water content (100%db.), DIC pretreatment with a pressurecomprised between 0.1 and 0.3 MPa and a short heating period offew seconds (5 to 45 s) combined to freezing and thawing allowsimprovement of drying/rehydration operations for apple with a goodpreservation of textural properties. DIC is considered as a goodalternative process to classical hot air drying and freeze-drying,especially for drying fragile fruit, such as strawberries (Alonzo-Macías, Cardador-Martínez, Mounir, Montejano-Gaitán, & Allaf, 2013).Furthermore, DIC coupled to hot air drying allows to preserve thenutritional value and bioactive molecules, at optimal DIC conditions(0.35 MPa for 10 s), treated strawberries were richer in anthocyaninsand phenolic compounds as compare to other classical drying methods.

DIC is recognized as a process for decontamination, debacterizationof foodstuffs. Three patents protect this application (Allaf, Debs-Louka,Louka, Cochet, & Abraham, 1994; Allaf et al., 1998). The treatmentallows DIC the elimination of micro-organisms (even in spore forms)through two main mechanisms: a controlled thermal treatment; pres-sure relaxation excessively stressed on microorganisms that cause theirexplosion (Debs-Louka, Louka, Abraham, & Allaf, 2010). Archeologicalinvestigations often renew pieces of wood having spent long periods inwater (mostly seawater). The DIC treatment can stop these degrada-tions and stabilize the archeologiocal waterlogged woods originatedfrom different museums (Allaf, Rezzoug, Cioffi, Louka, & Sanya, 1999;Sanya, Rezzoug, & Allaf, 1998). In the case of thermal treatment forallergen in peanuts, lentil, chickpeas and soybeans proteins, DICtreatment produces a reduction in the overall in vitro IgE binding.Immunoreactivity of soybean proteins was almost abolished with atreatment at 6 bars for 3 min. Additionally, DIC treatment (0.4 MPaduring 25 s) showed decrease in the IgE binding of whey proteins (β-lactoglobulin and α-lactalbumin) and a greater reduction of theallergenicity of whey proteins (Boughellout et al., 2015).

DIC pretreatment is considered an efficient method for extractionand texturing from various vegetal materials. Indeed, Mkaouar,Bahloul, Gelicus, Allaf, and Kechaou (2015) showed that DIC texturingon the solvent extraction of polyphenols from olive leaves improves theyield of extraction of 312% and permits generating extract richer inbioactive compounds. Another study has proved that DIC allowsenhancing lipid extraction from jatropha and rapeseed seeds withoutsignificant modification of fatty acids composition in comparison withconventional Soxhlet extraction (Nguyen Van, 2010). Allaf et al. (2014)have shown that enhancing of lipid extraction by DIC treatment isclearly noticed by calculation of effective diffusivity. DIC process is agood solution for deodorizing and expanse the vegetal matrix in thesame time before improving antioxidant extraction from rosemaryleaves (Allaf et al., 2013). Expansion of raw material permits a betterdiffusion of solvent through the material and accelerates the extractionof bioactive compound from 4 h for hydrodistillation to 3 min with DIC.More recently, DIC was endorsed as a pretreatment for in-situ transes-terification in the case of microalgae. Optimized DIC treatment(P = 0.16 MPa and t = 68 s) allows increasing of 27% in total lipidand> 75% in fatty acids methyl esters yield (Kamal, Besombes, & Allaf,2014). Additionally, to lipid extraction, it was observed that theresidual microalgae allow increasing of lutein extraction. Moreover,DIC allows reducing the energy consumption and manufacturing costcompared to conventional processes of lipid extraction.


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Table1

Exam

pleof

applications

andexpe

rimen

talco

nditions

ofDIC.

App

lications

Matrix

Expe

rimen

talco

nditions

Bene

fits

Referen

ce

Tran

sformation

Spray-drying

(spray

ingco

uplin

gto

DIC

andfina

ldrying

)

Milk

,sod

ium

caseinates

Whe

yproteinpo

wde

rs1)

Spraying

:T=

60–1

80°C,fi

nalp

owde

rshu

midity:

4an

d22

%db

.2)

DIC:P

=0.3–

0.7MPa

,t=

9–25

s3)

Drying:

50°C,a

irstream

1.2m/s

at26

5Pa

initial

humidity

Form

ationof

vacu

oles,which

increasedthe

specificsurfacearea

Better

func

tion

alqu

ality

Red

ucethespecificprob

lemsof

powde

rflow

ability

Improv

ingthekine

tics

offina

ldrying

(Mou

nir&

Alla

f,20

08)

Puffing (Hot

airdrying

andDIC

treatm

ent

coup

lingto

snak

ing)

Onion

chips

App

le1)

Drying:

T=

40°C,a

irflow

:1m/s,h

umidity:

267Pa

2)DIC

treatm

ent:P=

0.2–

0.6MPa

,t=

5–55

s(app

le)

P=

0.2–

0.5MPa

,t=

5–15

s(onion

)3)

Hot

airdrying

(sna

king

):T=

40°C,a

irflow

:1m/s,

humidity:

267Pa

,fina

lmoistureco

nten

t:5%

db.

Greater

effective

diffusivityan

dinitialstarting

accessibility

Expa

ndtheco

mpa

ctstructure

Vitam

inspreserva

tion

Low-cost,high

-qua

litysnak

ingan

dpo

wde

r

(Mou

niret

al.,20

11)

Texturation

(pre-dryingco

uplin

gDIC

andfreezing

)App

le1)

Pre-drying

at45

°C,2

m/s,fi

nalw

ater

conten

t:30

–200

%db

.2)

DIC:P

=0.1–

0.3MPa

,t=

5–45

s,3)

Freezing

:−30

°Cfor60

0min,a

fter

thaw

edat

4°C

Improv

emen

tof

drying

/reh

ydration

operations

Intensifying

theinternal

resistan

ceto

water

tran

sfer

Goo

dpreserva

tion

oftextural

prop

erties

(Ben

Haj

Said,B

ellagh

a,&Alla

f,20

15)

Swell-d

rying

(cou

plingDIC

tostan

dard

hotair

drying

)

Strawbe

rry

Green

Moroc

can

pepp

er

1)Pa

rtially

hotairdriedat

50°C

until18

%db

.,P v

apor=

265Pa

,air

flow

:1.2

m/s,t

=8h

2)DIC

cond

itions:P=

0.1–

0.6MPa

;t=

10–3

0s

3)Sa

meco

nditions

ofho

tairdrying

before

Efficien

ttech

niqu

eforfrag

ilefruit

Preserve

nutritiona

lva

lue

Improv

equ

ality

Decreaseco

nsum

eden

ergy

andco

ast

(Alonz

o-Macíaset

al.,20

13)

Preserva

tion

UHTde

contam

ination

(DIC

coup

lingto

hotairdrying

)Ba

cillu

sstearothermophilus

1)InitialDIC

stag

e:P=

0.7MPa

,5mm

thickdry,

t=3s

2)Heating

stag

e:T=

100–

150°C

t=5–

60s

Destruc

tion

ofmicroorga

nism

cellwallsan

dmore

specifically

onthesporewall

(Deb

s-Lo

ukaet

al.,20

10)

Con

servation

(suc

cessivepressure

drop

sde

hydration)

Arche

olog

ical

waterlogg

edwoo

d1)

Starch

impreg

nation

2)DIC

thermal

treatm

ent:T=

18–2

1°C

Endof

pressure

drop

T=

−1–

3°C

Smallshrink

age

Verygo

odsurfaceaspe

ctInitialco

lormaintain

Lower

moistureco

nten

tMorerapidthan

freeze-drying

(San

yaet

al.,19

98)

Thermal

treatm

entforallergen

(DIC

+solven

textraction

)Pe

anuts,

lentil,

chickp

eas,

soyb

eanproteins

1)DIC

treatm

ent:P=

0.3–

0.6MPa

,t=

1–3min,c

onstan

tinitialwater

conten

tof

50%db

.2)

Proteinextraction

withn-he

xane

Drastic

redu

ctionin

immun

oreactivity

Red

uction

intheov

erallin

vitroIgE

Timean

den

ergy

redu

ction

Goo

dalternativeto

intact

proteins

inthe

deve

lopm

entof

differen

tfood

prod

ucts

(Cua

drad

oet

al.,20

11)

Protein'sim

mun

oreactivity

Milk

P=

0.4MPa

T=

144°C

t=25

sPressure

drop

towards

5kP

a,32

°C

Enha

ncethean

tige

nicity

oftreatedcaseins

Decreasein

theIgE

(Bou

ghellout

etal.,20

15)

Extraction

Diffusion

(DIC

+solven

textraction

)Oliv

e(O

leaeuropa

eaL.)leav

es1)

DIC

pretreatmen

tco

nditions:

P=

0.1MPa

,num

berof

cycles

C=

1,t=

11s

2)So

lven

textraction

Destruc

tion

ofcellwalls

afterDIC

texturing

Intensification

ofsolven

textraction

(Mka

ouar

etal.,20

15)

Steam

extraction

(DIC)

Oak

woo

d(Q

uercus

alba

)ch

ips

P=

0.1–

0.6MPa

,t=

30– 3

00st=

5min

Initialmoistureco

nten

t:20

%,thickne

ssof

chips:

0.5mm

Deg

rada

tion

ofwoo

dcells

andsubseq

uent

rapid

liberationof

volatiles

Swellin

gan

dcreation

ofalve

oles

withinwoo

dmicrostructure

Econ

omyin

term

sof

timean

den

ergy

(Mellouk

,Meu

llemiestre,M

aach

e-Rezzo

ug,

Alla

f,&Rezzo

ug,2

013)

Deo

dorization

(DIC

+solven

textraction

)Rosem

aryleav

es1)

DIC

cond

itions:P=

0.6MPa

,tim

epe

rcycle:

6–40

s,nu

mbe

rof

cycle:

1–11

2)So

lven

textraction

Expa

nsionof

raw

materialindu

cing

abe

tter

extraction

ofan

tiox

idan

tStructural

alteration

seasedseco

ndarymetab

olite

extraction

(Alla

fet

al.,20

13)

(con

tinuedon

next

page)


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2.3. Success story

The technology of instant controlled pressure drop has beengenerated by Allaf group since 1988, several industrial projects havebeen developed. Many patents have been filed since 1993 (Allaf et al.,1994) and more than twenty PhD theses have treated the subject fromdifferent angles. Today, the Allaf group provides research whileparticipating in the design of machinery and the transition fromlaboratory studies to the industrial stage. The process is operated byABCAR-DIC Process company, localized in La Rochelle (France). Swell-drying is largely used at industrial scale to produce swell-dried productsof> 200 varieties such as apple, banana, strawberry, onion, tomatoetc. in the form of cubes, slices and powder that is found in healthy foodand unique bands known like “greedy snacking”, “fruit snacks” or“vegetable petals.” This process was also used for decontamination,dehydration and texturation of many foodstuffs. Furthermore, inter-mediate food products obtained after DIC treatment are used for thedevelopment of dehydrated meals or dairy products. The DIC technol-ogy is also largely used for the post-harvest rice processing. The USDAreport says that Egypt's rice paddy production in the year May 2012 toApril 2013 is expected to rise to 6.37 million tons of dried paddy rice,i.e., 4.5 million tons of dried unbroken white grain DIC rice. In China,many teabags treated by DIC have been commercialized and allow agreater diffusion of tea in water and even in cold water (Allaf & Allaf,2014).

3. Pulsed Electric Field

Pulsed Electric Field (PEF) treatment, also referred as electropora-tion or electropermeabilization, is a nonthermal process where anexternal electric field is applied to a living cell for a very short duration(from several nanoseconds to several milliseconds) (Fig. 3). The exactmechanism of membrane permeabilization is not precisely understoodyet, but it is accepted that electroporation consists of four differentstages including (Saulis, 2010): (a) increase of the transmembranepotential of the cytoplasmic membrane due to cell membrane chargingby the applied external electric field, (b) creation of small metastablehydrophilic pores if a threshold of transmembrane potential is reached(0.2–1.0 V), (c) evolution of the number and/or size of the createdpores during the PEF treatment, and (d) PEF post treatment stage withleakage of intracellular compounds, entrance of extracellular sub-stances i.e. as irreversible electroporation or pore resealing andintegrity recovering of membrane i.e. reversible electroporation.

The effectiveness of cell membranes electropermeabilization de-pends on several process parameters (electric field strength, treatmenttime, specific energy, pulse shape, pulse width, frequency and tem-perature), treatment mode (batch, continuous), configuration of treat-ment chamber (collinear, coaxial and parallel) (Van den Bosch, 2007),physicochemical characteristics of the treated matrix (pH and conduc-tivity), characteristics of the treated cells (size, shape, membrane, andenvelope structure) and state (suspension, solid, semi-solid)(Vorobiev & Lebovka, 2009).

PEF is a promising green tool in food processing as its opens a widerange of application due to the described phenomenon of cell mem-brane increased permeability or disruption via electroporation. Theapplication can be classified depending on the extent of the appliedexternal electric field and specific energy (Toepfl, Heinz, & Knorr,2006). For instance, the application of low electric treatment(E < 2 kV/cm; Q < 5 kJ/kg) is known to induce stress response onthe cellular level and is routinely used in molecular biology to gainaccess to the cytoplasm in order to introduce different molecules. Theapplications in this field are rather scarce and are limited to biologicalreaction enhancement of vegetable and microbial cells. The improve-ment of mass transfer is generally dependent on higher electric fields(0.1 < E < 50 kV/cm; 0.4 < Q < 60 kJ/kg). Food preservationdue to microbial or enzyme inactivation requires the highest level ofTa

ble1(con

tinued)

App

lications

Matrix

Expe

rimen

talco

nditions

Bene

fits

Referen

ce

Highe

rspecificsurfacearea

Tran

sesterification

insitu

(DIC

+Fo

lchextraction

)Microalga

e1)

DIC

cond

itions:P=

0.2–

0.6MPa

,t=

20–6

0s,

water

conten

t:30

and10

0%db

.2)

Mod

ified

conv

ention

alFo

lchextraction

Positive

lyaff

ects

porosity,d

iffusivityan

dlip

idav

ailability

Moresaferextraction

Quick

andeff

ective

proc

ess

(Kam

alet

al.,20

14)


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Fig. 3. Schematic view of a PEF treatment system with a representation of different types of treatment chambers and a brief description of electroporation phenomenon during the electrictreatment.

Table 2Example of applications and experimental conditions of PEF.

Application Matrix Treatment conditions Benefits Reference

PreservationInactivation Ringer solution

contaminated with B.subtilis spores

(PEF + heat)6 < E < 11 kV/cm;Q < 350 kJ/kg

Inactivation of spores with reduced heat load (Siemer, Toepfl, & Heinz, 2014)

Carrot puree (Chilling + PEF)0.1 < E < 1.1 kV/cm;0.15 < Q < 15.58 kJ/kg

Improvement of the stability of vitamin C andreduction of the residual activity of AAO andPOD

(Leong, Oey, Clapperton,Aganovic, & Toepfl, 2015)

Freezing/thawing Apple; spinach (PEF + impregnation + freezing+ thawing)0.58 < E < 0.8 kV/cm; Q: n.d.

Acceleration of freezing/thawing process andcomparable texture after defrosting to freshsamples

(Parniakov et al., 2016a; Phoon et al.,2008)

Osmoticdehydration

Apple, carrot (PEF + impregnation)0.22 < E < 10 kV/cm;0.15 < Q < 106.7 kJ/kg

Increase of water lossSolute uptake by the matrix depends on thematrix and operational conditions

(Rastogi et al., 1999; Wiktor et al.,2014)

Convective drying Carrot, red pepper (PEF + hot air drying)0.5 < E < 2.5 kV/cm;1.8 < Q < 56.5 kJ/kga

Increase of drying rates and color quality (redpepper)

(Gachovska et al., 2008; Won et al.,2015)

ExtractionDiffusion Grape pomace, sugar beet (PEF + extraction by diffusion)

0.6 < E < 3 kV/cm;Q < 19.4 kJ/kg

Increase of polyphenols and sucroseconcentration; selective extraction towardsanthocyanins, lower coloration and betterfiltrability of juices (sugar beet)

(Brianceau et al., 2015; Loginovaet al., 2011)

Expression Apple, grape (PEF + extraction by pressing)0.4 < E < 0.65 kV/cm;15 < Q < 32 kJ/kg

Increase of juice and polyphenol yield, decreaseof juice turbidity and better odor intensity

(Grimi, Lebovka,Vorobiev, & Vaxelaire, 2009; Turket al., 2012)

Filtration BSA suspension (PEF + cross flow UF)E = 4.5 kV/cm, Q: n.d.

Improvement of concentrating rate of protein inretentate and reducing the solute-relatedresistance to the permeate flux

(Robinson et al., 1993)

Distillation Roses (R. alba L.) E = 25 kV/cm, 10 < Q < 20 kJ/kg

Increase of oil essential oil yield and possiblereduce of distillation time

(Dobreva et al., 2010)

TransformationCutting Carrot E = 0.8 kV/cm, Q < 166 kJ/kg Decrease of the cutting force (Leong et al., 2014)Softening Meat 0.32 < E < 0.48 kV/cm; Q/n.d. Improving meat tenderness (Bekhit et al., 2016)Frying Potato 0.75 < E < 2.5 kV/cm; Q:

18.9 kJ/kgImproving potato color and reducing oil uptakeafter frying

(Ignat et al., 2015)

Fermentation S. cerevisiae 100 < E < 6 kV/cm; Q: n.d. Increase of sugars consumption, decrease offermentation time

(Mattar et al., 2015)

a Data not available in (Won et al., 2015).


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Version définitive du manuscrit publiée dans / Final version of the manuscript published in : Innovative Food Science and Emerging Technologies (2017), Vol. 41, p. 357-377, DOI: 10.1016/j.ifset.2017.04.016, Journal homepage : http://www.elsevier.com/locate/ifsettreatment (2 < E < 90 kV/cm; 50 < Q < 44,000 kJ/kg).

3.1. Food preservation

Food preservation (Table 2) is achieved whether by controlling orby inhibiting external contaminants and/or internal biological reactionsthat could alter the organoleptic and nutritional quality of food. Forthis, two main strategies are being used: a) applying thermal treat-ments; b) decreasing the water activity of the food matrix to inhibitbiological reactions.

Non-thermal PEF processing in liquid foods and beverages preserva-tion has been thoroughly studied as an alternative method to heatpreservation. A wide variety of vegetative microorganisms and enzymeshave been successfully treated in different food matrices(Griffiths &Walkling-Ribeiro, 2014; Martín-Belloso, Marsellés-Fontanet, & Elez-Martínez, 2014; Terefe, Buckow, & Versteeg, 2015).Better quality retention in PEF-processed products compared to thermalprocessing has been observed in many cases. However, PEF has oftenlittle or a limited effect on enzymes at processing conditions sufficientfor microbial inactivation (50–1000 kJ/kg). At sufficiently high-specificenergy input (e.g. > 1000 kJ/kg), PEF causes significant inactivationof enzymes at ambient and mild temperature conditions (Terefe et al.,2015). Commercial PEF treatment systems operate in continuous modefor high productivity. Generally, PEF treated liquid food is packagedafter their preservative treatment. A batch treatment mode, in con-ductive plastic material, could also be achieved with comparable levelsof inactivation (Roodenburg et al., 2013).

Depending on the required inactivation, target, product composi-tion and initial temperature, it may be advantageous to combine PEFtreatment with other treatments (heat, pH, antimicrobial). Suchcombinations may provide the required lethality at lower field strengthand with less electrical energy (Álvarez &Heinz, 2007).

Because of their rigid structures, bacterial spores can survive harshenvironments for a long period of time. The combination of tempera-ture and electric fields > 60 °C and 30 kV/cm respectively waseffective on spore inactivation (Siemer, Aganovic, Toepfl, & Heinz,2015).

The main strength seems to be in PEF ability to affect less thenutritional and sensory properties of food material as compared tothermal treatment. For instance, PEF treated beverages seem to havehigher contents of polyphenols, carotenoids and vitamins compared toheat pasteurization (Tokusoglu, Odriozola-Serrano, &Martín-Belloso,2014).

Freezing is a widespread method for food preservation. Unluckily,such treatment leads to deterioration of food texture and flavors duringsubsequent transformation operations. The formation, the size ofcrystals and recrystallization after freezing are the main reasons ofthe quality loss of frozen foods. Reversible electroporation, due to itstransient increase in membrane permeabilization, enables introductionof cryoprotectants into biological cells. This family of moleculesprevents crystal formation during freezing. This combination leads toa noticeable acceleration of the freezing/thawing process (Jalté,Lanoisellé, Lebovka, & Vorobiev, 2009; Parniakov, Bals,Lebovka, & Vorobiev, 2016a), increase of freezing temperature and adecrease of the ice propagation rate (Dymek, Dejmek,Galindo, &Wisniewski, 2015). Texture and firmness of spinach leaves(Phoon, Galindo, Vicente, & Dejmek, 2008), potato strips were retainedby impregnating the material with trehalose (Shayanfar, Chauhan,Toepfl, & Heinz, 2013) and apples with glycerol (Parniakov et al.,2016a).

Dehydration is probably the oldest means for food preservation. Theintact cell membranes in food materials represent a highly limitingfactor (barrier) to water transport during drying of food matrices. Poreformation during PEF treatment increases cell membrane permeabilitywhich enhances the mass transport phenomena. PEF treatment wassuccessfully combined with traditional processes such as osmotic

dehydration, freeze drying, radiant and convective heat. The resultsare encouraging as the combination of PEF and osmotic dehydrationresulted in an increase of water loss and migration of solutes into thefood matrix was observed (Rastogi, Eshtiaghi, & Knorr, 1999; Wiktor,Śledź, Nowacka, Chudoba, &Witrowa-Rajchert, 2014). A significantreduction of energy consumption and an acceleration of cooling anddrying time could also be achieved when apples and potatoes areelectrically treated prior to freeze drying without alteration of the driedsamples shape (Parniakov, Bals, Lebovka, & Vorobiev, 2016b;Wu & Zhang, 2014). Similar observations were reported for radiant(Baier, Bußler, & Knorr, 2015) and convective air drying (Gachovska,Adedeji, Ngadi, & Raghavan, 2008; Won, Min, & Lee, 2015). PEF treat-ment was beneficial to color quality of air-dried products (Won et al.,2015).

3.2. Extraction

Extraction by solvents (diffusion) and force fields (pressing, filtra-tion, and centrifugation) is widely used for production of liquid foodsand beverages as well as for extraction of molecules of industrialinterest. Pretreatments that modify the permeability of the cell mem-branes, such as grinding, heating, or enzymatic treatment, enhance themass transfer. However, these techniques may require a significantamount of energy and can cause losses of valuable food compounds.

The use of PEF became very popular in this field as it allows criticalacceleration of the solid–liquid extraction. Different technologies ofagro-industrial extraction become more selective and less energyconsuming if PEF is applied (Vorobiev & Lebovka, 2015).

The combination of PEF and extraction by diffusion has beeninvestigated for improving the extraction of different compoundslocated on the inside of plant cells, such as colorants (chlorophylls,carotenoids, betalains…), sucrose, polyphenols and other secondarymetabolites (Puértolas, Luengo, Álvarez, & Raso, 2012). PEF pretreat-ment can be applied for winemaking prior to the macerating fermenta-tion step, the extraction of polyphenols is improved and the wineresulting has different organoleptic (color) attributes (El Darra et al.,2016). The same pretreatment is applied to traditional wine makingresidues; an enhancement of the selectivity of colorant (anthocyanin)extraction is also highlighted (Brianceau, Turk, Vitrac, & Vorobiev,2015). PEF application has a large potential for replacement ormodification of the conventional thermal technology for sugar extrac-tion from sugar beets. PEF pretreatment assisted “cold” extractionresults in higher concentration of sucrose, lower concentration ofcolloidal impurities (especially, pectins), lower coloration and betterfilterability of juice (Loginova, Loginov, Vorobiev, & Lebovka, 2011).

Traditionally, the increase of the yield in the juice and oil extractionindustry has been one of the most important priorities. Gentletechniques that do not cause losses in nutritionally and organolepticattributes should be used in the procedures to improve the extractionyield. Different plant based matrix was successfully studied for pressureexpression combined with PEF pretreatments. Fruit juices (apple,grape…) and vegetable oils (olive) yield is significantly increased whenmoderate PEF treatments are applied before mechanical expression(Vorobiev & Lebovka, 2015). The electric treatment does not induce badflavors or taste in the oil (Abenoza et al., 2013) and can produce lessturbid, significantly odorant and high polyphenols content apple juices(Turk, Vorobiev, & Baron, 2012).

Pulsed Electric Field can also be combined with other mechanicalseparation operation such as filtration. The electric treatment helpsreducing the solute-related resistance to the permeate flux for concen-trating proteins. Significant improvements in the rate of concentratingthe protein in the retentate can be obtained, resulting in reducedmembrane surface area requirements for a specific degree of separation(Robinson et al., 1993).

The combination of PEF with extraction methods such as distillationis also a successive method that leads to an increase of essential oil yield


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and reduces the distillation time (Dobreva, Tintchev, Heinz,Schulz, & Toepfl, 2010).

3.3. Transformation

In addition to preservation and extraction applications, othermethods were proposed to enhance transformation processes in thelatest years. PEF is successfully applied to enhance the mechanicalremoval of undesired food parts. Skin removal of some fruits (tomato,mango…) gave results equal to steam peeling but with low appliedenergy (Toepfl, 2012). The data which are available on this topic arerather scarce.

Several studies have demonstrated interesting effects of PEF onsoftening vegetables and animal tissues. The viscoelastic and texturesproperties were changed after the electric treatment probably due toloss of turgor pressure (Lebovka, Praporscic, & Vorobiev, 2004). Thesemodifications have direct impact on decreasing the cutting force offruits (Leong, Richter, Knorr, & Oey, 2014) and improving meat tender-ness (Bekhit, Suwandy, Carne, Van de Ven, & Hopkins, 2016).

Several applications in preparation, curing and cooking of meat(McDonnell, Allen, Chardonnereau, Arimi, & Lyng, 2014) and vegetableproducts have also been proposed (Toepfl, Siemer, & Heinz, 2014). Forinstance, the application of moderate PEF treatment to potatoesimproves its color and reduces oil uptake after frying (Ignat,Manzocco, Brunton, Nicoli, & Lyng, 2015).

Low intensity PEF treatment, inducing reversible electroporation,was recently presented as stressing method to promote production ofmetabolites in vegetables or to accelerate biological reactions (Toepflet al., 2006). Mattar et al. (2015) showed that the electric treatmentprior to fermentation increases fructose consumption up to 3.98 timesat the end of the lag phase and 20 h decrease of the overall fermentationtime can be achieved compared to control (without electric treatment).

3.4. Success stories

The numbers of applications related to pulsed electric fields areconstantly increasing. New ideas are being tested in laboratory and atindustrial scale as reliable pulse modulators and tum-key systems.Recently, new PEF equipment manufacturers, such as Elea, Steribeam,Scandinova, and PurePulse, located in Germany, Sweden, and TheNetherlands, respectively, have emerged, thus indicating the growinginterest of the food industry in the application of the technology. Acooking device Nutri-Pulse® e-Cooker®, commercialized by IXLNetherlands B.V. is advertised as capable of preparing food with helpof electroporation and pulse ohmic heating, results in better conserva-tion of the original nutritive value and the original flavor, color,structure and taste.

4. Supercritical fluids

4.1. Principle, process and procedure

4.1.1. PrincipleSupercritical fluids (SCF) represent an alternative to organic sol-

vents in processes using solvents (Badens, 2012). A fluid is consideredto be in its critical state when it is both heated above its criticaltemperature (Tc) and pressurized above its critical pressure (Pc)(Brunner, 2005). The specificity of SCF relies in their physical proper-ties, which can be modulated by an increase of pressure and/ortemperature, beyond their critical values. SCF have a density close toliquids, which induces a solvating power close to liquids. Theirviscosity, close to gases and a diffusivity that is intermediary betweenliquids and gases, leads to an increase of mass transfer between thesolute to extract and the SCF. These properties enable adjustment ofsolvent selectivity of a SCF towards a target compound, which isparticularly interesting in the case of extraction.

Fig. 4. Simplified schematic representation of supercritical CO2 installation for solid extraction (A) and liquid extraction (B), example of supercritical fluid lab scale equipment – 1 Lautoclave (C).


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Supercritical CO2 (SC-CO2) is the fluid mostly used in SCF processes(Rozzi & Singh, 2002). Process implementation is eased due to its lowcritical coordinates (Tc: 31 °C, Pc: 7.38 MPa). Moreover, some of itsadvantages include non-inflammability, cheapness, abundance and itsvolatility at atmospheric pressure implies that after depressurizationextracts are solvent-free. SC-CO2 is a non-polar solvent; its solventpower is comprised between the one of pentane and toluene (Lumia,2011). To enhance solubilization of polar substances, a polar modifier(ethanol, methanol for example) can be added to SC-CO2.

4.1.2. Process implementationConcerning extraction and fractionation, two types of equipment

settings can be found. Supercritical fluid extraction (SFE) from solidmaterials is achieved with autoclaves (industrial units may be com-posed of several autoclaves for semi-continuous processing). Liquidfractionation with SCF is performed with countercurrent columns (forcontinuous processing).

SCF extraction installations for solid processing are composed offour main parts: (i) a volumetric pump, to ensure a correct pumping ofthe fluid, the pump can be preceded by a cooler which brings gaseouscomponent in a liquid state (ii) a heat exchanger, (iii) an extractor,where pressure is established and maintained by a back pressureregulating valve, (iv) a separator (Fig. 4A and C). Up to three separatorscan be put in series, to achieve multiple fractioning of the moleculescontained in the extracts.

Extraction by SCF from solids is divided in two main steps: theextraction and the separation of the solute from the solvent. To performSFE, the fluid has to be brought in its supercritical state. To achieve this,the fluid is usually sequentially pressurized and heated before enteringthe extractor. Brought at the desired pressure and temperature, the SCFpercolate in the extractor, with an ascending or descending flux. TheSCF extract the solute contained in the matrix. Separation of the solutefrom the SCF will be achieved in the separator, where the SCF will turninto a gaseous state, and the solute no longer solubilized in the SCF willbe separated by gravity. Extracts are therefore collected at the bottomof the separator. Depending on the equipment, the gas can be recycledby being re-injected in the system, or released to atmosphere.

Fractioning from a liquid feed can be performed in batch mode,where extraction is performed by desorption of a liquid placed on anabsorbent using the same equipment as for solid extraction (Benaissi,2013). In a continuous mode, a countercurrent column is used toselectively recover a solute from the feed (Fig. 4B). Regarding processimplementation, the feed is introduced in the middle or on the top ofthe column, the supercritical phase being introduced at the bottom ofthe column. The extract to be recovered and the fluid leave at the top ofthe column and the raffinate (heavier phase) is recovered at the bottomof the column. SCF preparation and regeneration are similar to SFEfrom solid material.

Apart from solid/fluid or fluid/fluid extraction processes, SCF areused for particle formation process and are the subject of extensivereviews (Jung & Perrut, 2001; Reverchon, 1999; Reverchon & Adami,2006; Rodríguez-Meizoso & Plaza, 2015). The general concept of twoprocesses is briefly described below:

RESS (Rapid Expansion of a Supercritical Solution). The solute ofinterest is diluted in a supercritical phase and the resulting mixtureis rapidly depressurized through a nozzle. This process has theadvantage to produce very fine solid particles, but its applicationsare limited by the polarity of the solutes to precipitate (low polaritysolutes).GAS or SAS (Gas or Supercritical fluid Anti Solvent) which conceptis to “decrease the solvent power of a polar liquid solvent in whichthe substrate is dissolved, by saturating it with carbon dioxide insupercritical conditions” (Jung & Perrut, 2001). This causes thesubstrate to precipitate or to recrystallize.

Compared to conventional processes, several key advantages resultfrom the use of SCF. Absence or limited solvent consumption (in thecase of co-solvent use) leads to production of a solvent-free extract. Thedepressurization step in supercritical fluid processes (SFP) enableslimiting the number of unit operations, since no separation or purifica-tion step is necessary. By operating at low temperatures during thewhole process, SFP are adapted to production of heat-sensitive biomo-lecules. Additionally, SCP are intrinsically sterile (Badens, 2012).

4.2. Applications in Green Food Processing

Since the 1970s, a great number of applications using SCF haveemerged and have been developed at laboratory and pilot scale. In thissection, some applications from published studies related to foodprocessing are reviewed, with a special emphasis on those dedicatedto transformation, preservation and extraction by SCF. Far from beingexhaustive, the examples given, when possible, will be supported bykey related reference reviews or papers.

4.2.1. TransformationTransformation processes can be achieved with the use of SCF, and

most of them are related to particle formation processes. Precipitationor crystallization of food compounds can be achieved by SAS-typeprocesses (e.g. carotenoids). To enhance biomolecules properties pre-servation, encapsulation with SCF has been investigated (Cocero,Martín, Mattea, & Varona, 2009; Rodríguez-Meizoso & Plaza, 2015).RESS and SAS processes have been successfully applied for anthocya-nins and antioxidant encapsulation (Table 3). Process performances aregenerally evaluated according to particle characteristics (size andmorphology), encapsulation efficiency and release of encapsulatedcompounds in a matrix.

Textural modifications of food matrix have been produced bycombining extrusion and SCF (Maskan & Altan, 2011; Rizvi,Mulvaney, & Sokhey, 1995). By injecting SC-CO2 during the extrusionprocess, the processing conditions are milder than conventional extru-sion (lower shear and starch expansion is possible below 100 °C).Therefore, torque, equipment wear and heat-sensitive compounddegradation can be minimized. Expansion of extrudates can be con-trolled according to the amount of SC-CO2 injected, improving thestructural characteristics of extrudates (Table 3).

Fractioning by SCF is used for aroma fractioning, where waxes(compounds of high molecular weight) can be separated from thevolatile fraction or for lipid fractionation from oils (Reverchon, 1997).Fractioning can be performed after extraction in the depressurizationstages through the separators or with a countercurrent column.Fractional extraction can also enable a selective recovery of compounds(Table 3, Palma, Taylor, Varela, Cutler, & Cutler, 1999).

The use of SCF for micronization of particles for food applicationshas been described by Weidner (2009). Production of powdered foodsuch as chocolate or lecithin at different particle size can be obtainedthrough RESS, SAS and PGSS (Particle from Gas Saturated Solutions)(Weidner, 2009).

4.2.2. PreservationFood preservation aims at conserving organoleptic properties and

guarantees safety in food consumption. Food deterioration may becaused by several factors such as micro-organisms development andendogenous enzymatic activity. The use of SCF or high pressure gasesfor preservation by sterilization, for microbial, virus and spore inactiva-tion has been the subject of some extended reviews (Garcia-Gonzalezet al., 2007; Perrut, 2012; Spilimbergo, Elvassore, & Bertucco, 2002).

High hydrostatic pressure has been known to enable sterilizationand pest control (Perrut, 2012), but the required pressure is quite highe.g. between 2 and 3000 bars (Spilimbergo et al., 2002). Requiringmilder conditions for similar results, the use of SCF appears as a suitablealternative for food preservation. Early studies reported that relatively


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Table3

App

lications

ofsupe

rcriticalfluids

infood

tran

sformation,

preserva

tion

andextraction

.

App

lication

Matrix(targe

tmolecule)

Proc

essing

cond

itions

Bene

fits

Referen

ce

Tran

sformation

Encapsulation

Jabu

ticaba

skins

(antho

cyan

ins)

RES

Sproc

ess

P CO2:2

00ba

rs,4

0°C,c

o-solven

t:EtOH,e

ncap

sulation

inpo

lyethy

lene

glycol

79.78%

encapsulationeffi

cien

cyStab

ility

ofan

thoc

yanins

tolig

htan

dtempe

rature,ease

ofdissolutionin

solven

t

(San

tos,

Albarelli,

Bepp

u,&Meireles,

2013

)

Rosem

ary(antioxida

nts)

SASproc

ess

P CO2:8

0to

100ba

rs,2

5to

50°C,solve

nt:E

tOH,e

ncap

sulation

inpo

loxa

mers(Pluronic®

F88or

Pluron

ic®F1

27)

100%

encapsulationeffi

cien

cyQuick

dissolutionin

aque

oussolution

(1h),inc

reased

protection

againstde

grad

ationfactorsdu

ring

dissolution.

(Visen

tin,

Rod

rígu

ez-Rojo,

Nav

arrete,

Maestri,&

Coc

ero,

2012

)

Fraction

ation

Orega

no,sage

,thy

me,

marigold(essen

tial

oils)

Extraction

:PCO2:3

00ba

rs,4

0°C

Fraction

ationin

sepa

rators

(S):10

0ba

rs(S1)

and50

bars

(S2)

Sepa

ration

ofwax

esin

firstsepa

ratoran

dmax

imal

reco

very

ofessentialoilob

tained

inseco

ndsepa

rator(>

70%)

(Forna

ri,V

icen

te,V

ázqu

ez,G

arcía-

Risco

,&Reg

lero,2

012)

Grape

seed

(phe

nolic

andlip

idco

mpo

unds)

Fraction

1:pu

reCO2(456

bars,3

5°C,1

5min

static,d

ynam

icph

ase:

solven

tto

feed

ratio:

16.6)

Fraction

1:CO2+

metha

nol(5:1,v/

v)(456

bars,35

°C,

15min

static,d

ynam

icph

ase:

solven

tto

feed

ratio:

16.6)

Fraction

1:co

mpo

sedof

fattyacids,

alipha

ticalde

hyde

san

dsterols(10.6%

yield)

Fraction

2:ph

enolic

compo

unds

7.9%

yield(catechin,

epicatechinan

dga

llicacid).

(Palmaet

al.,19

99)

Textural

mod

ification

Cornan

dpo

tato

(extruda

teprod

uction

)SC

FXproc

esswithwhe

ypo

wde

r/eg

gwhite

inco

rporation.

Die

tempe

rature:6

0°C,s

crew

speed:

100rpm,d

ieCO2pressure:

100to

150ba

rs

Enha

nced

expa

nsion,

redu

ctionof

starch

degrad

ationan

dho

mog

eneo

usmicrocellu

larstructureco

mpa

redto

steam

extrud

ates

(Alavi,G

ogoi,Kha

n,Bo

wman

,&Rizvi,1

999)

Whe

atflou

rSC

FXproc

ess,

twin

screw

extrud

er,D

ietempe

rature:8

0°C,

screw

speed:

300to

400rpm,d

ieCO2pressure:10

bars

CO2injectionallowed

lower

proc

essing

tempe

raturesan

dredu

cedloss

ofthiamine(3

to11

%ag

ainst10

to16

%)an

dlower

water

absorption

inde

x.

(Sch

mid,D

olan

,&Ng,

2005

)

Crystalliz

ation/

precipitation

Lyco

pene

SASproc

ess,

P CO2:7

to15

0ba

rs,3

5to

45°C,s

olve

nt:

dich

lorometha

neYieldsab

ove95

%Increasing

pressure

lead

sto

increase

ofpa

rticle

size

andhigh

erinitialco

ncen

trationlead

sto

smallerpa

rticles.

(Migue

l,Martín,

Gam

se,&

Coc

ero,

2006

)

Shrimpresidu

es(astax

anthin)

SASproc

ess,P C

O2:1

00to

120ba

rs,3

5to

40°C,solve

ntto

feed

ratio:

1,solven

t:aceton

e,co

-precipitation

withPluron

ic®F1

2774

%en

capsulationeffi

cien

cy,h

ighe

rco

lorpreserva

tion

compa

redto

crud

eextract

(Mezzo

moet

al.,20

12)

Preserva

tion

Bacteria

inactiva

tion

Escherichiacoli(carrot)

P CO2:1

20ba

rs,3

5°C,1

0min

Non

detectab

leleve

ls(G

alva

ninet

al.,20

14)

Listeria

mon

ocytogenes

(dry

curedha

m)

P CO2:1

20ba

rs,5

0°C,2

5min

Non

detectab

leleve

ls(G

alva

ninet

al.,20

14)

Sporeinactiva

tion

Alicycloba

cillu

sacidoterrestris

(app

lejuice)

P CO2:8

0ba

rs,70

°C,3

0min

Non

detectab

leleve

ls(Bae,L

ee,K

im,&

Rhe

e,20

09)

Bacillu

ssubtilis(suspe

nsion)

P CO2:80ba

rs,3

5°C,3

0min

(30cycles)

Com

pleteinactiva

tion

(Spilim

bergoet

al.,20

02)

Enzymeinactiva

tion

Polyph

enol

oxidase

(red

beet)

P CO2:7

5ba

rs,55

°C,3

0min

93%

loss

ofactivity

(Liu

etal.,20

10)

Pectinesterase

(orang

ejuice)

P CO2:2

69ba

rs,5

6°C,1

45min

100%

loss

ofactivity

(Balab

anet

al.,19

91)

Drying

Carrot

P CO2:2

00ba

rs,4

0°C

to60

°C,5

0min

to15

min,c

o-solven

t:EtOH

(6%

mol)

Microstructurean

dshap

eco

nserva

tion

,favo

rablerehy

drated

textural

prop

erties

(Brown,

Frye

r,Norton,

Baka

lis,&

Bridson,

2008

)

Extraction

Percolation

Tomatowastes(lycop

ene)

P CO2:3

44ba

rs,8

6°C,2

00min

61%

extraction

oflyco

pene

(Roz

zi,S

ingh

,Vierling,

&Watkins,2

002)

Alm

ond(oil+

toco

pherols)

P CO2:3

50to

550ba

rs,3

5to

50°C,1

0to

30kg

/h,m

axim

umreco

very

at2to

3hof

extraction

Highe

sttoco

pherol

enrich

men

tin

oilo

btaine

din

thefirst2

hof

extraction

.Co-extraction

oftoco

pherol

andoilfavo

redat

the

high

estpressurestested

.

(Leo

,Rescio,

Ciurlia,&

Zach

eo,20

05)

Liqu

id/liquidextraction

Soyb

eanoil(lecithin)

GASC

proc

ess,

P CO2:5

0to

65ba

rs,2

4.85

°C,s

oybe

anoil

dilutedin

95%

hexa

neEn

rich

men

tof

98.6%

oflecithin

insolid

prod

uct

(Muk

hopa

dhya

y&Sing

h,20

04)

Prop

olis

tinc

ture

(essen

tial

oil

andflav

onoid)

SASproc

ess,

P CO2:3

00ba

rs,60

°C,o

ptim

umtinc

ture

conc

entration:

10%

mass

100%

reco

very

offlav

onoids

(Catch

pole,G

rey,

Mitch

ell,&La

n,20

04)

Pressing

Coc

oanibs

(oil)

GAMEproc

ess,

P CO2:1

00ba

rs,10

0°C,e

ffective

mecha

nical

pressure:5

00ba

rs87

.1%

oilrecov

eryag

ainst71

.8%

oilrecov

eryforco

nven

tion

alpressing

atthesameexpe

rimen

talco

nditions

(Ven

teret

al.,20

06)

Linseeds

(oil)

GAMEproc

ess,

P CO2:1

00ba

rs,40

°C,e

ffective

mecha

nical

pressure:1

00ba

rs30

%increase

usingGAMEproc

essby

compa

ring

with

conv

ention

alpressing

atthesameexpe

rimen

talco

nditions

(Willem

set

al.,20

08)

Filtration

Carrotoil(beta-carotene

)31

0ba

rs,4

0to

60°C,Δ

P:30

to50

bars,m

embran

esare

nano

filters

Perm

eate

enrich

men

tin

beta-caroten

e(from

9.4up

to24

.2pp

m)

(Sarrade

etal.,19

98)

GAME:

Gas

AssistedMecha

nicalEx

pression

,GASC

:Gas

Anti-So

lven

tCrystalliz

ation,

P CO2:C

O2pressure,RES

S:Rap

idEx

pansionof

aSu

percriticalSo

lution

,SAS:

Supe

rcriticalAnti-So

lven

t,SC

FX:S

upercritical

FluidEx

trusion.


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Version définitive du manuscrit publiée dans / Final version of the manuscript published in : Innovative Food Science and Emerging Technologies (2017), Vol. 41, p. 357-377, DOI: 10.1016/j.ifset.2017.04.016, Journal homepage : http://www.elsevier.com/locate/ifsetmild conditions were sufficient to inhibit the growth and increase theinactivation rate (heat treatment of 50 to 55 °C with 6 bars of CO2)(Fraser, 1951; Perrut, 2012). Generally, the microbial inactivation isgreatly affected by pressure, temperature, exposure duration andcompression/decompression cycles (Garcia-Gonzalez et al., 2007;Melo Silva et al., 2013; Perrut, 2012; Spilimbergo et al., 2002). Thepresence of water is reported to increase the bactericidal effect of CO2,most probably due to its relationship with pH, where acidic pH tends tofavor inactivation (Garcia-Gonzalez et al., 2007; Garcia-Gonzalez et al.,2009). Some other authors investigated the positive effect of condensedgases (e.g. CO2, N2) on microorganisms inactivation. However, it mustbe underlined that the matrix effect plays a major role during theinactivation process (Garcia-Gonzalez et al., 2007; Wei, Balaban,Fernando, & Peplow, 1991). Recent investigations on food matrices(Table 3) report that inactivation can be obtained with moderateconditions (CO2 pressure between 80 and 120 bars and below 70 °C).Such conditions enable a complete inactivation or no detectable levelsin foods such as carrots, cured ham, apple and orange juice and red beetafter treatment.

Enzyme inactivation can be obtained when exposed to SC-CO2

conditions or dense phase conditions. Reported factors leading toenzyme inactivation are pH lowering and inhibitory effect of molecularCO2. In that sense, although inactivation can be achieved with othersgases, CO2 is suggested to have a unique role in inactivation(Damar & Balaban, 2006). At very mild conditions (between 1 and100 bars at temperatures below 60 °C), inactivation of enzymes such aspectin esterase and polyphenol oxidase can be achieved(Damar & Balaban, 2006). It was noted that some enzymes such aslipoxygenase and peroxidase in sucrose solutions required higherpressures for inactivation (100 to 600 bars, below 55 °C) so someenzymes are more pressure-sensitive than others (Hendrickx,Ludikhuyze, Van den Broeck, &Weemaes, 1998; Tedjo,Eshtiaghi, & Knorr, 2000). Early studies report the use of CO2 micro-bubbles in batch and continuous systems for enzyme inactivation inliquid materials such as fruit juices (Ishikawa, Shimoda,Shiratsuchi, & Osajima, 1995; Ishikawa et al., 1997;Wimmer & Zarevúcka, 2010).

4.2.3. ExtractionExtraction by SCF is well-known at both academic and industrial

level and therefore is the subject of numerous publications. Four typesof processes related to extraction are presented in Table 3.

Supercritical extraction of natural products (such as oils and fats,antioxidants, pigments and aromas) by percolation is described inseveral reviews (Díaz-Reinoso, Moure, Domínguez, & Parajó, 2006;Herrero, Cifuentes, & Ibañez, 2006; Reverchon, 1997; Reverchon &DeMarco, 2006). From literature survey, it can be identified that usuallyhigh pressures are required (above 280 bars) for extraction of highmolecular weight compounds such as oils. Aromatic fractions such asessential oils are extracted using moderate conditions (pressures from70 to 200 bars and temperatures from 40 to 60 °C) (Reverchon, 1997;Sovová, Aleksovsk, Bocevska, & Stateva, 2006). Focus in extraction bypercolation is also set on by-product valorization or on the use of SCFfor co-extraction of compounds for enhancement of final productattributes (Table 3). Liquid-liquid extraction is applied for numerousapplications such as concentrated aromas production from beveragesand alcohol removal (Brunner, 2005; Macedo et al., 2008), oilfractionation and deodorization (Shimoda et al., 2000; Torres,Torrelo, Señoráns, & Reglero, 2009), and hexane removal from vege-table oils (Eller, Taylor, & Curren, 2004). Processing pressures rarelyexceed 300 bars.

Combined processes with SCF have been investigated to increaseextraction performances. A process combining pressing and use of gasesin a supercritical state (Gas Assisted Mechanical Expression, GAME) hasbeen recently investigated to increase oil extraction yield (Voges,Eggers, & Pietsch, 2008). This process has been successfully applied

on various seeds (cocoa, linseeds, sesame, Table 3). Authors havenoticed that pressing was greatly favored by SCF or dense gases, indeeda low mechanical pressure is necessary (around 10 MPa) to increase oilyield from 10 to 20% (all other conditions equal) (Venter, Willems,Kuipers, & Haan, 2006; Willems, Kuipers, & de Haan, 2008). Nano-filtration coupled to SC-CO2 extraction for the purification of lowmolecular weight compounds (1500 g·mol−1) was introduced bySarrade, Rios, and Carlès (1998). This process has been applied topurification of beta-carotene from carrot oil and to fractionation of fishoil triglycerides. Further developments on combination of membranetechnologies and SCF are still on going in the field of edible oil refining(Temelli, 2009).

4.3. Success story in the use of supercritical fluids: industrial production

Industrial processing with SCF has been a reality for several years.Since early patents on coffee decaffeination or hops extraction in the1970′s, a great number of industrial units have emerged. In 2009,Perrut estimated that 300 industrial units were using SCF. For super-critical extraction performed on solid materials, the main applicationsare related to food and perfume industry: aromas and flavors extraction(hops, vanilla, ginger, roses…), coffee and tea decaffeination. Forexample, Maxwell House Coffee (a division from General Foods) hasreported processing 80,000 tons of coffee per year. The plant isequipped with a 60 m3 extractor and to function in a semi-continuousscale (Benaissi, 2013). The removed caffeine is further sold to pharma-ceutic or food companies.

5. Microwave extraction

5.1. Process and procedure

Microwave heating results from the dissipation of the electromag-netic waves in the irradiated medium. The dissipated power in amedium depends on the dielectric properties and the local time-averaged electric field strength. So, there is a fundamental differencebetween microwave and conventional heating: in conventional heating,heat transfers occur from the heating device to the medium, whereas inmicrowave heating, heat is dissipated inside the irradiated medium. Incontrast with conventional heating, microwave heat transfer is notlimited to thermal conduction or convection currents (Fig. 5). Inpractice, this means that a much faster temperature increase can beobtained. Furthermore, the maximum temperature of the materialheated by microwaves is only dependent upon the rate of heat lossand power applied.

Although microwaves create volumetric heating, the field distribu-tion is not even throughout the irradiated material. Therefore, theenergy is not homogeneously dissipated. The electric field distributiondepends on the geometry of the heated object and the dielectricproperties. For media which readily absorb microwaves, the depth atwhich power density is reduced to 1/e of original intensity might be alimiting factor.

For more transparent media, the occurrence of standing wavepatterns will result in ‘hot spots’ if the power dissipation is faster thanthe heat transfers to surrounding colder areas. As a general rule astanding wave pattern can occur if multiples of a half wavelength fit inthe typical dimension (d) of the irradiated object.

Microwave ovens can have monomode or multimode cavity. Themonomode cavity can generate a frequency which excites only onemode of resonance. Their use for food processing is limited because thevolume has to be extremely small in order to maintain the resonance.The majority of food heating applications (Edgar & Osepchuk, 2001)use a multimode resonance cavity applicator because it permits largevolumes. The incident wave is able to affect several modes ofresonance, and this superimposition of modes allows the homogeniza-tion of field.


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Microwaves are only absorbed by dipoles, transforming their energyinto heat. Heat transfer advantages of applying microwave power, anon-contact energy source, into the bulk of a material include: faster

energy absorption, reduced thermal gradients, selective heating andvirtually unlimited final temperature. Several processes such as drying,tempering, thawing, blanching, sterilization, pasteurization, baking and

Fig. 5. (a) A brief description of phenomenon in the cell generated by microwave irradiation, (b) microwave tunnel to temper, reproduced with permission from SAIREM, (c) microwavecooking of desserts in containers, reproduced with permission from SAIREM, (d) microwave tunnel for pasteurization of liquid food, reproduced with permission from MES Technologies,(e) microwave extraction: SFME and MHG, reproduced with permission from Millestone.

Table 4Example of applications and experimental conditions of MW.

Application Matrix Treatment conditions Benefits Reference

PreservationPasteurization Kiwifruit puree P: 1000 W, t: 200 s and P: 900 W, t:

225 s; m: 500 gInactivation 90% of peroxidase enzyme Benlloch-Tinoco, Martínez-

Navarrete, & Rodrigo, 2014Thawing Strawberries P: 700 W, t: 10 min, m: 250 g A reduction in processing time,

No influence on the quality indices (color, ascorbicacid and anthocyanins contents)

Holzwarth, Korhummel,Carle, & Kammerer, 2012

Sterilization Palm fruit P: 800 W, t: 2 min Increment in lauric acid (C12: 0),Highest concentration of vitamin E and carotenecontent,Clean technology due to zero water effluent discharge

Cheng, Mohd Nor, & Chuah, 2011

ExtractionMHG Grape juice by-

productsP: 400 W, t: 20 min, m: 400 g Green extraction method,

Efficiency of MHG in the extraction of polyphenols andanthocyanins from grape by-products

Al Bittar, Périno-Issartier,Dangles, & Chemat, 2013

SFME Lavender flowers P: 500 W, t: 10 min Extraction of essential oilsShort extraction time

Chemat et al., 2006

MHG Rosmarinusofficinalis L.

P: 500 W, t: 15 min Extraction of antioxidantsEconomy in term of time and energyMore safer extraction

Abert Vian, Fernandez,Visioni, & Chemat, 2008

TransformationDrying bananas P: 400 W, magnetron is « on » for

11 s and « off » for 18 s, m: 86 g.Creation dried-and-crisp fruits by applying successivecycles of heating and vacuum pulses in a microwavefield

Monteiro, Carciofi, & Laurindo, 2016

Baking Cake batter P: 250 W, t: 67 s, m: 30 g of freshlyprepared batter

93% reduction in baking time/convective bakingImprovement textural properties such as moisturecontent and firmnessHighest nutritive value

Megahey et al., 2005

Blanching Brussels sprouts P: 700 W, t: 5 min followed byblanching in boiling water for2 min.

No deleterious effects on total flavonoids and ascorbicacid,Improvement health properties of Brussels sprouts

Vina et al., 2007


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Version définitive du manuscrit publiée dans / Final version of the manuscript published in : Innovative Food Science and Emerging Technologies (2017), Vol. 41, p. 357-377, DOI: 10.1016/j.ifset.2017.04.016, Journal homepage : http://www.elsevier.com/locate/ifsetextraction have been applied efficiently in the food industry.

5.2. Applications in food processing (Table 4)

Drying is one of the oldest methods of preserving food and can bespecified as a simultaneous heat and mass transfer operation in whichwater activity of a foodstuff is lowered by the removal of water byevaporation into an unsaturated gas stream. The most importantcharacteristic of microwave dehydration is volumetric heating effectwhere the microwave energy travels through the food and is absorbedmore in the wet region than in the dry region of the product.Consequently, the centre is warmer than the surroundings and themass transfer is accelerated. Microwave drying results in a high thermalefficiency, shorter drying time and improves the final quality of thedried product compared to conventional drying. MW drying is also ableto maintain good quality of the product such as color, aroma andtexture (Fathima, Begum, & Rajalaksmi, 2001).

Several experimenters have reported microwave-assisted hot-airdrying experiments with foodstuffs, where considerable improvementsin the drying process have been evident such as better aroma, faster,and better rehydration (Gowen, Abu-Ghannam, Frias, & Oliveira, 2006)than hot-air drying.

Quality can often be improved further by the addition of vacuum:Vacuum Microwave Drying (VMD) offers an alternative way to retainvolatile compounds sensitive to losses through thermal and oxidativedegradation. Moreover, the absence of air during drying reducesoxidation and therefore, color, texture and nutrient content of productsare all improved (Gunasekaran, 1999). The VMD technique was alsosuccessfully applied to cranberries, (Yongsawatdigul & Gunasekaran,1996) model fruits gels (Drouzas, Tsami, & Saravacos, 1999), garlic(Cui, Xu, & Sun, 2003), cabbages (Yangyang, Mujumdar, Le-qun, & Jin-cai, 2004) and button mushrooms (Giri & Prasad, 2006).

In addition to hot air, microwaves can also be combined with freezedrying. Freeze drying is used for heat sensitive product and almost nooxygen is involved in the process. However, this technique is costly,time and energy consuming. In this system, the energy is directlyabsorbed by the water molecules for sublimation within the materialand increases the drying rate in freeze drying.

Blanching is a thermal treatment prior to freezing with the aim ofinactivation of enzymes such as polyphenoloxidase (PPO) and perox-idase (POD) that are responsible for browning reactions and lead to off-flavor development. Blanching also destroys microorganisms on theproduct surface and makes some vegetables more compact. Microwaveblanching could be an alternative to conventional blanching, withprecise process control, shorter processing time and less energy use anddecreases the blanching time of the product centre. Many studiesconcluded that the microwave technique leads to firmer products,equal or better nutrient contents and similar colors when compared toconventional processing (Brewer & Begum, 2003; Lin & Brewer, 2005).

Tempering can be considered as the initial phase of the completethawing process. Thawing of frozen foods is an important unitoperation in the food industry. Large quantities of food have to bepreserved by freezing at harvest time for use throughout the year. Inmicrowave thawing, electromagnetic waves are directly absorbed bythe product without the use of conductors or electrodes. Therefore, it isa very fast thawing method but its application is limited by productthermal stability. The problem is complex because the water loss factoris approximately 12 whereas that of ice is 0.003, which means that theice is almost insensitive to microwave energy. In a frozen product(−18 °C), unfrozen water preferentially absorbs the microwave energywhereas the frozen part is insensitive to microwaves. This leads tolocalized areas of very hot water, partial thawing and thermal runaway(Schiffmann, 2001). Improvements to maintain a uniform temperatureduring microwave thawing are necessary.

The advantage of microwave thawing was the reduction in proces-sing time, even when there was no significant effect on product quality.

In the food industry, microwave ovens are often part of continuousprocesses. Thin layers of product circulate on a conveyor under asuccession of microwave generators. Microwaves are used to thaw fishfillets and meat blocks.

Microwave tempering reduces costs of manufacturing preparedfoods as frozen raw materials can be tempered as needed, with no driploss, without the need for tempering rooms and reduced processingtime.

Baking is a complex process, described as a simultaneous heat andmass transfer. Baking involves a series of physical, chemical andbiochemical changes in food, such as starch gelatinization, proteindenaturation, carbon dioxide liberation from leavening agents, volumeincrease, water evaporation, crust formation and non-enzymatic brown-ing (Therdthai & Zhou, 2003).

Microwave baking reduces the baking time and energy (Sumnu,2001). Megahey, Mcminn, and Magee (2005) illustrated this bycomparing the time to bake a cake by microwave and conventionalbaking. Microwave baking allowed for up to a 93% reduction in bakingtime, relative to convective baking. Cakes baked by microwavesshowed improved textural properties such as moisture content andfirmness. Another advantage of microwave baking is that the finalproduct has a higher nutritive value.

Pasteurization is a thermal inactivation of pathogenic microorgan-isms, notably vegetative cells, yeasts and moulds. Sterilization is theinactivation of microorganisms and their spores, which are generallymore thermo-resistant than vegetative cells. The microwave heating offood provides an excellent opportunity to pasteurize or sterilize theproducts. Products such as sweet mash potato (Coronel, Truong,Simunovic, Sandeep, & Cartwright, 2005; Steed et al., 2008), a biphasicfood product (salsa con queso) (Kumar, Coronel, Simunovic, & Sandeep,2007), green beans and mash carrot (Kumar et al., 2008), were treatedand the feasibility of microwave sterilization was confirmed. Thecontinuous pasteurization and sterilization of liquids with microwaveequipment are a useful alternative processing approach but the priceand the energy consumption are relatively high.

5.2.1. ExtractionUse of microwave energy was described for the first time in 1986 by

Ganzler (Ganzler, Salgo, & Valko, 1986) and Lane (Lane & Jenkins,1984) for extraction of food ingredients. In the last decade there hasbeen an increasing demand for new extraction techniques, amenable toautomation, with shortened extraction times and reduced organicsolvent consumption, to prevent pollution and reduce the cost ofsample preparation. Driven by these goals, advances in microwavegreen extraction have given rise to two classes of techniques: SolventFree Microwave Hydrodistillation and Microwave Hydrodiffusion andGravity.

Solvent Free Microwave Hydrodistillation (SFME) was conceivedfor laboratory scale applications in the extraction of essential oils fromdifferent kinds of aromatic plants and fruits (Chemat, Lucchesi, andSmadja (2004a, 2004b)) SFME apparatus is an original combination ofmicrowave heating and distillation at atmospheric pressure. Based on arelatively simple principle, this method involves placing plant materialin a microwave reactor, without any added organic solvent or water.The internal heating of the in situ water within the plant materialdistends the plant cells and leads to rupture of the glands and oleiferousreceptacles. Thus, this process frees essential oil which is evaporated bythe in situ water of the plant material. A cooling system outside themicrowave oven condenses the distillate continuously. The water excessis refluxed to the extraction vessel in order to restore the in situ water tothe plant material. Therefore, the SFME method offers a reducedenvironmental burden as it rejects less CO2 in atmosphere (200 g CO2

per gram of essential oil compared to traditional method which wasrejecting 3600 g CO2 per gram of essential oil) (Chemat et al., 2004a,2004b; Ferhat, Meklati, Smadja, & Chemat, 2006).

Microwave Hydrodiffusion and Gravity (MHG) extraction was


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Version définitive du manuscrit publiée dans / Final version of the manuscript published in : Innovative Food Science and Emerging Technologies (2017), Vol. 41, p. 357-377, DOI: 10.1016/j.ifset.2017.04.016, Journal homepage : http://www.elsevier.com/locate/ifsetpatented by Chemat et al., 2008. This green extraction technique is anoriginal “upside down” microwave alembic combining microwaveheating and earth gravity at atmospheric pressure. MHG was conceivedfor laboratory and industrial scale applications for the extraction offood ingredients from different kind of fruits, vegetables and aromaticplants. This method involves placing plant material in a reactor insidethe microwave oven, without adding any solvent or water. Microwavesinduce warming of the water contained in the matrix, which allows thedestruction of cells containing essential oil. Essential oils, as well as theinternal water of the matrix, are released and transferred from inside tothe outside of the plant: this is the hydrodiffusion phenomenon. Acooling system placed outside the microwave oven allows the con-densation of the distillate. It is important to note that this green methodallows extract of essential oils without distillation and evaporationwhich are the most energy consuming processes between the unitoperations (Périno-Issartier, Giniès, Cravotto, & Chemat, 2013).

5.3. Success story

Using microwaves, full reproducible food processes can now becompleted in seconds or minutes with high reproducibility, reducingthe processing cost, simplifying manipulation and work-up, givinghigher purity of the final product, eliminating post-treatment of wastewater and consuming only a fraction of the time and energy normallyneeded for a conventional processes heated by convection, conduction,or radiation. For food production, the resultant value could include:more effective heating, fast heating of packaged food, reduced equip-ment size, faster response to process heating control, faster start-up,increased production, and elimination of process steps.

6. Ultrasound assisted food processing

Ultrasound is a sound frequency in the range between 18 and100 kHz that is above hearing of the human ear. High power ultrasoundmeans application of intensities higher than 1 W·cm−2 (usually in therange between 10 and 1000 W·cm−2). High power and low frequencyultrasound (f = 20 to 100 kHz) is considered as “power ultrasound”because its application causes cavitation and is applied in the foodindustry (Paniwnyk, 2005). The benefits of US are attributed to acousticcavitation: micro-bubbles created in a liquid phase when subjecting amixture to US will grow and oscillate quickly before collapsing due topressure changes (Chemat et al., 2008; Jambrak, Mason, Lelas,Herceg, & Herceg, 2008) (Fig. 6a). These violent implosions will frag-ment or disrupt the surface of the solid matrix, enhancing mass transferand accelerating diffusion.

The effectiveness of the ultrasound depends to the acousticfrequency, temperature and pressure applied. Lower frequencies gen-erate larger bubbles and thus a more violent bubble collapse withhigher localized temperatures and pressures. However, as frequency isincreased, there are more collapse events per unit time. Two differenttypes of ultrasound equipment are commonly used in laboratory(Fig. 6). The first one is the ultrasonic cleaning bath (Fig. 6b) whichis commonly used for solid dispersion into solvent (ultrasounds willdramatically reduce the size of the solid particles, which will enhanceits solubility), for degassing solutions or even for cleaning smallmaterial by immersion of the glassware into the bath. The ultrasonicbaths are less used for chemical reactions even if they are easy to handleand economically advantageous because reproducibility of reaction islow. In fact, the delivered intensity is low and is highly attenuated bythe water contained in the bath and the walls of the glassware used forthe experiment. The second one, the ultrasonic probe or horn system(Fig. 6d), is much more powerful because the ultrasonic intensity isdelivered on a small surface (only the tip of the probe) compared to theultrasonic bath. Another change is that the probe is directly immersedinto the reaction flask so less attenuation can happen. This system ofprobe is widely used for sonication of small volumes of sample but

special care has to be taken because of the fast rise of the temperatureinto the sample. A special sono-extraction reactor (from 0.5 to 3 L) hasbeen developed by REUS (www.etsreus.com, FRANCE) (Fig. 6c) Theintensity of ultrasounds is about 1 W/cm2 with a frequency of 25 kHz.In order to keep constant temperature, the reactor is made of a doublemantle into which cooling water can circulate. The main advantage ofthis type of apparatus is that the natural products and the extractionsolvent are mixed into a container and the ultrasounds are directlyapplied to the mixture. To run out industrial trials or to scale-uplaboratory experiments, REUS has also developed reactors from 30 to1000 L (Fig. 6f, g). Pump systems are coupled to the ultrasonic bath inorder to fill the ultrasonic bath, to stir the mixture and to empty thesystem at the end of the experiment. The manufacturers of high-powerultrasound equipment have been also focusing on designing devices byincluding specific operational features such as continuous flow mode.The equipment basically consists of a glass tube or stainless steelreactor, through which the fluid mixture is pumped, surrounded by ajacket filled with pressurized water for conduction of the sound waves.Ultrasound is transmitted to the system by a sonotrode attached to thejacket (Fig. 6e).

6.1. Application in food processing

There are a large number of potential applications of high intensityultrasound in food processing of which a number are discussed below(Table 5).

6.1.1. Degassing/deaerationA liquid contains gases as a mixed condition, such as dissolved

oxygen, carbon dioxide, nitrogen gas etc. Two common methods usedfor degassing are boiling and reducing pressure while ultrasound has anadvantage in the small temperature change. Degassing in an ultrasonicfield is a highly visible phenomenon when ultrasound, e.g. an ultrasoniccleaning bath, is used with regular tap-water inside. It occurs when therapid vibration of gas bubbles brought them together by acoustic wavesand bubbles grow to a size sufficiently large to allow them to rise upthrough the liquid, against gravity, until they reach the surface(Laborde, Bouyer, Caltagirone, & Gerard, 1998; Tervo,Mettin, & Lauterborn, 2006). Several acoustic cavitation structuresgenerated in low-frequency ultrasound fields within the range(20–50 kHz) have been investigated and these have been summarizedby Mettin (2005). In the food industry, this technique can be used todegas carbonated beverages such as beer (defobbing) before bottling(Brown &Goodman, 1965).

6.1.2. DemoulingGenerally, the industrial cooking of foods leads to adhesion of the

products to the cooking vessel or in other operations it must detachfrom its mould. At present, to solve this problem mechanical methodssuch as knocking vibration are used to remove the products. Analternative solution to these conventional methods is to release foodproducts by coupling the mould to a source of ultrasound (Scotto,1988). The device for demoulding industrial food products couples themould and the ultrasonic source in order to enhance removal of theproduct contained in the latter by virtue of the high-frequency relativemovement between the contact surfaces of the mould and of theproduct contained in the latter. This technique allows surface coatingsto be eliminated and ensures that any residual material in the mouldcan be cleaned automatically.

6.1.3. CuttingThe introduction of ultrasound in food cutting has improved the

performance of overall food processing. Ultrasonic food cutting equip-ment provides a new way to cut or slice a variety of food products thatstreamlines production, minimizes product waste and lowers mainte-nance costs. Ultrasonic cutting uses a knife-type blade attached through


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a shaft to an ultrasonic source (Rawson, 1988). The cutting tool itselfcan be of many shapes and each shape can be considered to be anacoustic horn, part of the whole ultrasonic resonating device. Cuttingwith the superimposition of ultrasonic vibration is a direct competitorof technologies such as high-velocity water jet cutting and conventionaltechniques such as using saws or knives. The low energy requirementsfor ultrasonic cutting have been presented (Schneider, Zahn, & Rohm,2008; Schneider, Zahn, Schindler, & Rohm, 2009). The ultrasoniccutting characteristics depend on the food type and condition, e.g.frozen or thawed (Brown, James, & Purnell, 2005). The most wide-spread application of ultrasound is in the cutting of fragile foodstuffs. Ituses in the particular cases of fragile and heterogeneous products(cakes, pastry and bakery products) and fatty (cheeses) or stickyproducts (Arnold, Leiteritz, Zahn, & Rohm, 2009).

6.1.4. Meat tenderizationThe quality of meat depends on the aroma, flavor, appearance,

tenderness and juiciness. Consumer behaviour has shown that tender-ness is most important palatability factor in determining meat quality(Smith, Cannon, Novakofski, McKeith, & O'Brien, 1991). The traditionalmethod used for meat tenderization is mechanical pounding, whichmakes poorer quality meat more palatable. Power ultrasound has alsobeen found to be useful for this process. Ultrasound can act in two ways:by breaking the integrity of muscular cells or by enhancing enzymaticreactions, i.e. via a biochemical effect (Boistier-Marquis, Lagsir-Oulahal, & Callard, 1999). A pilot study involving sirloin steak(Roberts, 1991) showed that sonicating beef muscle at 2 W·cm2 for2 h at 40 kHz produced damage to the perimysial connective tissue,resulting in improved eating texture.

6.1.5. Food preservationMicroorganisms and enzymes are the primary factors responsible of

food deterioration. Conventional thermal processing kills vegetativemicroorganisms and some spores, and inactivates enzymes. However,

the time and temperature of the process are proportional to the amountof nutrient loss, development of undesirable flavors and deterioration offunctional properties of food products. Ultrasound is one of the newpreservation techniques that could eliminate microbial activity. Highpower ultrasound alone is known to disrupt biological cells. Whencombined with heat treatment, it can accelerate the rate of sterilizationof foods. Therefore, it reduces both the duration and intensity of thethermal treatment and the resultant damages. At sufficiently highacoustic power inputs, ultrasound is known to rupture cells (Chisti,2003; Chisti &Moo-Young, 1986; Dakubu, 1976). A cell can beinactivated at an intensity less than that needed to cause disruption.The mechanism of microbial killing is mainly due to the thinning of cellmembranes, localized heating and production of free radicals(Butz & Tauscher, 2002). There are many examples of microorganismsinactivated using ultrasound. Some of these have been studied inculture media and others in food, using ultrasound either combinedor alone. The most frequently studied microorganisms, not only in thefield of power ultrasound, but also among other methods of foodpreservation are Saccharomyces cerevisiae and Escherichia coli. Theformer has been found to be less resistant to ultrasound than othervegetative cells, which is mostly attributed to its larger size. Theinactivation of this microorganism has been proven in such foodmodels as water, phosphate buffers, and sabouraud broth (Ciccolini,Taillandier, Wilhem, Delmas, & Strehaiano, 1997; Guerrero, Lopez-Malo, & Alzamora, 2001; Petin, Zhurakovskaya, & Komarova, 1999).The inactivation of Staphylococcus aureus, Pseudomonas fluorescens,Listeria monocytogenes and E. coli has been proven in water andphosphate buffers, as well as in foods such as UHT milk. Ultrasonicationin combination with heat was performed to study the inactivation ofListeria innocua and mesophilic bacteria in raw whole milk. Whenapplying ultrasound in combination with heat the kill rates wereincreased when compared to rates of thermal treatment alone and asynergistic rather than an additive effect was observed. Ultrasoundproduced a good level of inactivation under different treatment

Fig. 6. a) Acoustic cavitation, b) ultrasonic bath, c) sono-extractor by REUS, d) ultrasonic probe, e) continuous ultrasonic probe system, f) industrial ultrasonic equipment (500 L), g)industrial ultrasonic equipment (50 L).


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Table5

Exam

pleof

applications

andexpe

rimen

talco

nditions

ofUS.

App

lication

Matrix

Treatm

entco

nditions

Bene

fits

Referen

ce

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tion

Inactiva

tion

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ejuice

500kH

z,24

0W,1

5min

Inactiva

tion

oftotalmesop

hilic

aerobe

san

dfung

iValeroet

al.,20

07

Milk

24kH

z,40

0W,5

5°C,2

,5min

Inactiva

tion

ofListeria

inno

cua

Noc

i,Walkling-Ribeiro,C

ronin,

Morga

n,&Ly

ng,2

009

Phosph

atebu

ffer

20kH

z,10

0W,4

0–61

°C,1

00–5

00kP

a,0,25

-4min

Inactiva

tion

ofEscherichiacoli

Lee,

Zhou

,Lian

g,Fe

ng,&

Martin,

2009

Extraction

Polyph

enolic

compo

unds

Van

illin

Citruspe

el

Van

illapo

ds

USba

th,6

0kH

z,15

°C–4

0°C,2

g/40

,80%

metha

nol,

1h

USho

rn,2

2.4kH

z1hpu

lsed

mod

e(5

s.ON/5

sOFF

)1g/

100mLsolven

t

Highe

rextraction

efficien

cyby

USco

mpa

redto

maceration.

Low

extraction

tempe

rature

lead

sto

high

eryields.

140pp

mva

nillinco

ncen

trationin

1hvs

180pp

min

8hco

nven

tion

alSo

xhlet

Barbero,

Liazid,Pa

lma,&Ba

rroso,

2008

Jadh

av,Rek

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ogate,&Ratho

d,20

09

Lyco

pene

Tomatoe

sUSba

th,4

0kH

z,30

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g/8mLof

ethy

lacetate,

sonicatedfor29

min

at86

°C;

90%

totallyco

pene

extractedin

29min,y

ield

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gUSwith

microwav

esLian

gfu&Ze

long

,200

8

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sformation

Cutting

Che

ese

Guillo

tine

sono

trod

e,40

kHz,

cuttingve

locity

2500

mm.m

in−

1an

dultrason

icam

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μm.

Adv

antage

s:Fa

ster,m

oreeffi

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-deformationof

theprod

ucts.

Thekn

ifeis

self-clean

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icswhich

aretran

smittedfrom

the

gene

rator.

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al.,20

09

Deg

assing

Meattend

erization

Milk

Jumbo

squid

20kH

z,pu

lsed

ultrasou

nd(1

s/1s),2

0°C,3

min

25.6

kHz,

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0.8min

Effective

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efoam

anddissolve

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ygen

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milk

Tend

erizationof

jumbo

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isingtheothe

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The

pred

ictedva

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ofthetexture,

includ

ingtheflexibility

andthefirm

ness,w

ere2.40

mm

and43

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respective

ly.

Villam

iel,Verdu

rmen

,&de

Jong

,200

5

Huet

al.,20

14


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conditions and media for Bacillus species. The inactivation of Listeriamonocytogenes by high-power ultrasonic waves (20 kHz) at ambienttemperature and pressure has been found to be low with decimalreduction values in 4.3 min. This could be improved however either byan increase in pressure (manosonication) or by increasing the power ofsonication. Inactivation by manothermal sonication (MTS) proved to bemore effective (Manas, Pagan, Raso, Sala, & Condon, 2000; Pagan,Manas, Alvarez, & Condon, 1999).

For stabilization of some food materials, enzymes must be inacti-vated or their activity reduced. Enzyme inactivation can be easilyachieved by heat treatment. However, in some cases the high heatresistance of enzymes may be a problem as heat can negatively modifysome food properties such as flavor, color or nutritional value. This isthe driving force for the increased interest in an alternative method ofenzyme inactivation: high power ultrasound, i.e. sonic waves above20 kHz. The effects of ultrasonic waves on proteins are very complex.Polymeric globular proteins are broken down into subunits and ifoxygen is present, the quaternary structure is not recoverable. A partialdelipidation of lipoproteins can be obtained and if the ultrasonicirradiation is long enough, proteins can be hydrolysed and polypeptidechains can be broken. The influence of the gas on the intensity ofenzyme inactivation has been related to the formation of free radicalsby cavitation. Sensitivity to ultrasounds depends on the conditions ofthe treatment (McClements, 1995) as well as on the nature of theenzyme. Generally, ultrasonication in combination with other treat-ments is more effective in food enzyme inactivation. In fact, MTStreatment has an increased effectiveness compared with ultrasoundalone (Manas et al., 2000). MTS treatments inactivate several enzymesat lower temperatures and/or in a shorter time than thermal treatmentsat the same temperatures.

6.1.6. ExtractionUltrasound assisted extraction is an emerging potential technology

that can accelerate heat and mass transfer and has been successivelyused in extraction field. Ultrasound waves after interaction withsubjected plant material alter its physical and chemical propertiesand their cavitational effect facilitates the release of extractablecompounds and enhances the mass transport by disrupting the plantcell walls. Ultrasounds are successively employed in plant extractionfield. Several classes of food components such as aromas, pigments,antioxidants, and other organic and mineral compounds have beenextracted and analyzed efficiently from a variety of matrices (mainlyanimal tissues, food and plant materials). Riera et al. (2004) examinedthe effect of ultrasound (20 kHz and 50 W) on the particulate almondoil extraction kinetics using supercritical CO2. As a consequence of thetrials (at 280 bar and 55 °C) at the end of the extraction time (8 h30 min) the yield of the oil was significantly increased (20%) when SFEwas assisted by ultrasound. Alternatively, mass transfer was speeded upto such an extent that yields comparable to those obtained by SFE alonecould be achieved in about 30% shorter time when using ultrasound.

6.2. Success stories

The considerable interest in high-powered ultrasound is due to itspromising effects in food processing and preservation, such as higher

product yields, shorter processing times, reduced operating and main-tenance costs, improved taste, texture, flavor and color, and thereduction of pathogens at lower temperatures. It can be applied notonly to improve the quality and safety of processed foods but offers thepotential for developing new products with unique functionality aswell. Nevertheless, although conventional cutting, emulsification andcleaning are often bottlenecks, lack of knowledge keeps industry fromimplementing ultrasound in their processes.

A recent survey and market study of the possible future applicationsof new process technologies (like microwave, ultrasound) in the foodindustry has revealed that many companies are reluctant to apply thesenew technologies. The main reason is poor understanding of these newtechniques by food professionals and the reason or weight of tradition.

7. Comparison of techniques

The use of innovative extraction techniques such as ultrasound,microwave, instant controlled pressure drop, supercritical fluid, andpulsed electric fields (Table 6) allows reduced extraction time, energyconsumed, and less water or solvent. Conventional techniques arelimited by the diffusion of water or solvent into biomass, due to rigidstructure of cell walls of microorganisms. The solution could be toenhance the diffusion of water or solvent and to disrupt cell walls. Forexample, ultrasound and electric pulse fields allow in a high disruptionof cell, which permits accelerating the mass transfer, thus, processingtime is reduced. In another hand, heating by microwave inducescombined mass and heating transfer that permits the destruction ofcells and liberation of metabolites. As a future trend is to have adecision tool which permits selecting a technology regarding the initialmaterial. For example, the choice of which technique has to be used toperform extraction of a desired metabolite from a specific plant has tobe a result of a compromise between the efficiency and reproducibilityof extraction, ease of procedure, together with considerations of cost,time, safety and degree of automation.

Another challenge for the food industry in the coming years, such asconsumer and society demand on one side high quality, safe, nutritionalprocessed foods but also in another side reduction of waste andawareness about climate change. Environmental studies are difficultin particular with food products. Ideally a complete LCA study shouldnecessarily include agricultural production, industrial refining, storageand distribution, packaging, consumption and waste management,which comprise large and complex systems (Sonnemann and Margni(2015); Peano et al. (2012); Pardo and Zufía (2012).).

8. Conclusions and perspective

Food processing even preservation, transformation or extractiontakes an important place in manufacturing processes and is linked toseveral drivers such as request for naturally derived ingredients (colors,antioxidants, antimicrobial, aromas…) by the consumers, and the needof standardization. Green Food Processing could be a research thematicthat encompasses a comprehensive strategy based on the discovery andthe design of processes in order to reduce energy and water consump-tion. It has been investigated mainly at laboratory scale by severalresearch teams in Europe mostly, and represents a good opportunity to

Table 6Characteristics, main disadvantages and advantages of green extraction techniques.

Technique Investment Sample size Processing time Main disadvantages Main advantages

Ultrasound Low 600 L Low Problem for separation High cell disruptionMicrowave Medium 150 L Low Hot spots Cell disruptionDIC High 100 L Low High energy consumption High cell disruptionSFE High 300 L Medium Need of know-how Enhance mass transferPEF High Continuous Medium Difficult ease of operation Electroporation of wall cells


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rationalize eco-friendly developmental and industrial practices.The food industry is a very competitive environment and to survive

they have to use optimized processes and to reduce the carbon foodprint. The concept of Green Food Processing meets the demand of thefinal consumer in term of greener product, an education work will haveto be done in order to explain what the benefits are for the finalconsumer. This educational work will require vulgarization from thescientific community and industry members and avoid the shortcuts of“green washing”. For example, in Avignon University to illustrate anapplication of Green Food Processing in teaching laboratories, we usedgreen procedures employing ultrasound energy and microwave energyas energy source to teach fundamental food processing concepts such asmarinating, maceration and extraction. As an example, we havedeveloped new green procedure, using microwave energy as energysource, to teach the fundamental concepts of extraction of essential oilsused for aromatisation of food products. The objective of this teachingwas to offer students the opportunity to compare the potential of thisgreen technique for extraction of essential oil with a traditional hydro-distillation method (used in all the teaching laboratories all over theworld) and to appreciate the benefits of using greener processingmethod: reduction in time, energy and water consumption. These greenfood-processing techniques could be easily understood by youngerpeople. Each year, we open our research laboratory during the openweek of “La fête de la science” and show the innovations about

processing food especially extraction of food ingredients (aromas,colors…) with original techniques such as microwave and ultrasound(Fig. 7).

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Fig. 7. Practical work on Green Food Processing for Master students at AvignonUniversity and Introduction to green extraction for primary schools at Avignon University


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Version définitive du manuscrit publiée dans / Final version of the manuscript published in : Innovative Food Science and Emerging Technologies (2017), Vol. 41, p. 357-377, DOI: 10.1016/j.ifset.2017.04.016, Journal homepage : http://www.elsevier.com/locate/ifsetBoughellout, H., Choiset, Y., Rabesona, H., Chobert, J. M., Heartle, T., Mounir, S., ...

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